EP3190088B1 - Verfahren für ammoniaksynthese - Google Patents

Verfahren für ammoniaksynthese Download PDF

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Publication number
EP3190088B1
EP3190088B1 EP15837863.8A EP15837863A EP3190088B1 EP 3190088 B1 EP3190088 B1 EP 3190088B1 EP 15837863 A EP15837863 A EP 15837863A EP 3190088 B1 EP3190088 B1 EP 3190088B1
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EP
European Patent Office
Prior art keywords
ammonia
gas
raw material
ammonia synthesis
synthesis
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EP15837863.8A
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English (en)
French (fr)
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EP3190088A1 (de
EP3190088A4 (de
Inventor
Mikiya Sakurai
Yukio Tanaka
Naoya OKUZUMI
Hiroyuki Osora
Haruaki Hirayama
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Mitsubishi Heavy Industries Engineering Ltd
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Mitsubishi Heavy Industries Engineering Ltd
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Publication of EP3190088A4 publication Critical patent/EP3190088A4/de
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00—Ammonia; Compounds thereof
    • C01C1/02—Preparation, purification or separation of ammonia
    • C01C1/04—Preparation of ammonia by synthesis in the gas phase
    • C01C1/0405—Preparation of ammonia by synthesis in the gas phase from N2 and H2 in presence of a catalyst
    • C01C1/0458—Separation of NH3
    • C01C1/047—Separation of NH3 by condensation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/002—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by condensation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
    • B01J23/46—Ruthenium, rhodium, osmium or iridium
    • B01J23/462—Ruthenium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00—Ammonia; Compounds thereof
    • C01C1/02—Preparation, purification or separation of ammonia
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00—Ammonia; Compounds thereof
    • C01C1/02—Preparation, purification or separation of ammonia
    • C01C1/04—Preparation of ammonia by synthesis in the gas phase
    • C01C1/0405—Preparation of ammonia by synthesis in the gas phase from N2 and H2 in presence of a catalyst
    • C01C1/0411—Preparation of ammonia by synthesis in the gas phase from N2 and H2 in presence of a catalyst characterised by the catalyst
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/02—Materials undergoing a change of physical state when used
    • C09K5/04—Materials undergoing a change of physical state when used the change of state being from liquid to vapour or vice versa
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25B—REFRIGERATION MACHINES, PLANTS OR SYSTEMS; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS
    • F25B9/00—Compression machines, plants or systems, in which the refrigerant is air or other gas of low boiling point
    • F25B9/002—Compression machines, plants or systems, in which the refrigerant is air or other gas of low boiling point characterised by the refrigerant
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/56—Platinum group metals
    • B01J23/58—Platinum group metals with alkali- or alkaline earth metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/56—Platinum group metals
    • B01J23/63—Platinum group metals with rare earths or actinides
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts

Definitions

  • the present invention relates to an ammonia synthesis method capable of improving an operating efficiency of ammonia synthesis.
  • ammonia (NH 3 ) is synthesized from hydrogen (H 2 ) and nitrogen (N 2 ) as raw materials in an ammonia synthesis column.
  • NH 3 ammonia
  • N 2 nitrogen
  • this ammonia synthesis when ammonia is separated from a synthetic gas in an ammonia synthesis loop, and a product ammonia is taken out as a liquid, a cooling process using a chiller refrigerant is used in general.
  • an ammonia synthesis method comprising a step of synthesizing ammonia gas from a raw material gas in an ammonia synthesis reactor comprising a Ru-based catalyst, a step of water-cooling the synthetic gas obtained from the reactor using a gas cooler, and a step of separating the cooled synthetic gas into an ammonia-containing gas and an ammonia-containing liquid in three consecutive ammonia separators, wherein the ammonia-containing gas leaving the third ammonia separator has an ammonia concentration of 0.08 mol%.
  • the ammonia-containing gas is returned to the ammonia synthesis reactor by mixing it with nitrogen and hydrogen so as to provide a raw material gas, compressing the raw material gas in circulating compressor, pre-heating the compressed raw material gas using a heat exchanger, and introducing the pre-heated compressed raw material gas into the ammonia synthesis reactor (Patent Literature 3).
  • an object of the present invention is to provide an ammonia synthesis method capable of reducing refrigerant manufacturing cost without using a product ammonia as a chiller refrigerant and improving an operating efficiency of ammonia synthesis.
  • the invention is defined by the claims.
  • the invention thus relates to an ammonia synthesis method including an ammonia synthesis step of synthesizing an ammonia gas from a raw material gas for ammonia synthesis, wherein an ammonia synthesis catalyst that synthesizes the ammonia gas is a ruthenium catalyst, a water-cooled or air-cooled cooling step of water-cooling or air-cooling a synthetic gas containing the obtained ammonia gas and an unreacted raw material gas, an ammonia separation step of separating the synthetic gas after cooling into the ammonia gas and a liquid ammonia, and a compression step of compressing a return raw material gas when the raw material gas containing the separated ammonia gas is returned to the ammonia synthesis step side as the return raw material gas, wherein an ammonia concentration in the return raw material gas to be introduced into the ammonia synthesis step is 5 mol% or more and the temperature of the synthetic gas after cooling is from 30 to 50°C.
  • an operating efficiency of ammonia synthesis can be improved without using a product ammonia as a chiller refrigerant unlike conventional art.
  • FIG. 1 is a schematic diagram of an ammonia synthesis system for carrying out the ammonia synthesis method of the invention.
  • FIG. 2 is a schematic diagram of another ammonia synthesis system for carrying out the ammonia synthesis method of the invention.
  • the ammonia synthesis system 10A includes an ammonia synthesis column 13 that synthesizes an ammonia gas 12A from a raw material gas (hydrogen (H 2 ) and nitrogen (N 2 )) 11 for ammonia synthesis, a discharge line L 11 that discharges a synthetic gas 14 containing the ammonia gas 12A obtained from the ammonia synthesis column 13 and an unreacted raw material gas 11A, a water-cooled cooler 16 that cools the synthetic gas 14 with a coolant 15, disposed in the discharge line L 11 , an ammonia separator 17 to which the discharge line L 11 is connected, into which a synthetic gas 14A after cooling is introduced and which separates the ammonia gas 12A and a liquid ammonia 12B from each other, a raw material return line L 12 that returns a raw material gas containing the ammonia gas 12A separated by the ammonia separator 17 to the ammonia synthesis column 13 side as a return raw material gas 11B, and a compressor 18 that compress
  • An ammonia concentration in the return raw material gas 11B to be introduced into the ammonia synthesis column 13 is 5 mol% or more, and an ammonia synthesis catalyst that synthesizes the ammonia gas 12A in the ammonia synthesis column 13 is a ruthenium catalyst.
  • the ammonia synthesis system 10A is constituted by connecting the ammonia synthesis column 13 containing an ammonia synthesis catalyst to the ammonia separator 17 using the discharge lines L 11 and the raw material return line L 12 to form an ammonia synthesis system circulation loop.
  • the ammonia synthesis column 13 synthesizes an ammonia gas from a raw material gas 11 (and the return raw material gas 11B) with an ammonia synthesis catalyst.
  • a ruthenium (Ru) catalyst is used as the ammonia synthesis catalyst used in the ammonia synthesis column 13.
  • the ruthenium catalyst means a catalyst containing 0.1 wt% or more of ruthenium, and preferably contains, in addition to ruthenium as a main component, a promoter of at least one element selected from the group consisting of an alkali metal (for example, sodium (Na), potassium (K), rubidium (Rb), or cesium (Cs)), an alkaline earth metal (for example, magnesium (Mg), calcium (Ca), strontium (Sr), or barium (Ba)), and a rare earth element (from lanthanum of the element number 57 to lutetium of the element number 71).
  • a promoter of at least one element selected from the group consisting of an alkali metal (for example, sodium (Na), potassium (K), rubidium (Rb), or cesium (Cs)), an alkaline earth metal (for example, magnesium (Mg), calcium (Ca), strontium (Sr), or barium (Ba)
  • a rare earth element from lanthan
  • alkali metal as a promoter examples include sodium (Na), potassium (K), rubidium (Rb), and cesium (Cs).
  • alkaline earth metal examples include magnesium (Mg), calcium (Ca), strontium (Sr), and barium (Ba).
  • the rare earth element examples include lanthanum of the element number 57 to lutetium of the element number 71.
  • a relationship among a synthesis pressure, a cooling temperature, and a synthesis temperature preferably has a relationship of "ammonia equilibrium concentration at outlet of ammonia synthesis column ⁇ operating pressure"> "ammonia partial pressure at inlet of ammonia synthesis column”.
  • the pressure is preferably in a range of 7 to 25 MPa, and more preferably in a range of 10 to 20 MPa.
  • the synthesis reaction temperature is preferably in a range of 200°C to 600°C.
  • a H 2 /N 2 ratio is preferably in a range of 1 mol/mol to 5 mol/mol.
  • the cooling temperature is in a range of 30°C to 50°C as described below.
  • the ammonia gas 12A is synthesized from the raw material gas 11 with an ammonia synthesis catalyst, and is discharged as the synthetic gas 14 from the ammonia synthesis column 13 through the discharge line L 11 .
  • the ammonia gas 12A and the unreacted raw material gas 11A are mixed in the synthetic gas 14.
  • the water-cooled cooler 16 warer-cools the synthetic gas 14 synthesized in the ammonia synthesis column 13 with the coolant 15.
  • the coolant 15 has a temperature width in summer and winter, but the temperature of the synthetic gas 14A after cooling is about from 30 to 50°C.
  • an air-cooled cooler 22 as illustrated in FIG. 2 may be used in place of cooling with the water-cooled cooler 16.
  • the air-cooled cooler 22 that cools the synthetic gas 14 is disposed in the discharge line L 11 that discharges the synthetic gas 14 from the ammonia synthesis column 13.
  • the air-cooled cooler 22 air-cools the synthetic gas 14 passing therethrough by introducing air 21 thereinto with a fan 22a.
  • the air 21 has a temperature width in summer and winter, but the temperature of the synthetic gas 14A after cooling is from 30 to 50°C.
  • the ammonia separator 17 separates the ammonia in the synthetic gas 14A after water-cooling or air-cooling into the ammonia gas 12A and the liquid ammonia 12B, and performs gas-liquid separation, for example, by a vapor-liquid separating drum.
  • the liquid ammonia 12B which has been subjected to gas-liquid separation by the ammonia separator 17 is separately recovered as a product ammonia by a product ammonia line L 13 .
  • the ammonia gas 12A and the unreacted raw material gas 11A are returned as the return raw material gas 11B to the ammonia synthesis column 13 side by the raw material return line L 12 .
  • the return raw material gas 11B is compressed to a predetermined pressure set for ammonia synthesis by the compressor 18 disposed in the raw material return line L 12 .
  • a make-up gas line L 14 that introduces the raw material gas 11 as a make-up gas is connected to the raw material return line L 12 so as to be joined with the raw material return line L 12 prior to the compressor 18 between the ammonia separator 17 and the ammonia synthesis column 13 so as to obtain a predetermined synthesis concentration.
  • a compressor 20 that compresses the raw material gas 11 newly supplied is disposed in the make-up gas line L 14 .
  • the synthetic gas 14 introduced into the ammonia separator 17 has been cooled to 10°C or lower with a refrigerant (for example, ammonia refrigerant).
  • a refrigerant for example, ammonia refrigerant
  • cooling is performed only with the coolant 15 or the air 21 without using any refrigerant, and the temperature of the synthetic gas 14A after cooling is set to 30 to 50°C. Therefore, the return raw material gas 11B in the ammonia separator 17 that separates the liquid ammonia 12B contains a large amount of the ammonia gas 12A.
  • the ammonia concentration in the return raw material gas 11B to be introduced into the ammonia synthesis column 13 is 5 mol% or more, or more (for example, 10 mol% or more) according to temperature and pressure conditions.
  • FIG. 3 is a diagram illustrating a relationship between an inlet ammonia concentration (mol%) introduced into the ammonia synthesis column 13 and an ammonia synthesis rate (kmol/(h ⁇ m 3 )).
  • the solid line indicates a ruthenium (Ru) catalyst
  • the one dot chain line indicates an iron (Fe) catalyst.
  • the iron catalyst reduces the synthesis rate immediately when the concentration of ammonia exceeded 5 mol%.
  • the ruthenium catalyst is highly active even with a high concentration of ammonia (for example, 10 to 15 mol%), and such a large reduction as in the iron catalyst was not observed.
  • the conventional iron catalyst reduces the reaction rate of ammonia synthesis, and therefore requires a larger amount of the catalyst, but use of the ruthenium catalyst does not reduce the synthesis rate, and requires a smaller catalyst amount than the iron catalyst.
  • Table 1 indicates comparison between the present invention and a conventional example.
  • the present invention uses the coolant 15 or the air 21. Therefore, the cooling temperature of the synthetic gas 14A after cooling, introduced into the ammonia separator 17 is from 30 to 50°C.
  • the conventional example uses a chiller refrigerant, and therefore the cooling temperature is 10°C or lower.
  • an inlet NH 3 concentration (mol%) of the ammonia synthesis column (reactor) 13 was 10 mol% because of a large amount of return ammonia gas.
  • an inlet NH 3 concentration (mol%) of the ammonia synthesis column (reactor) 13 was 5 mol% because of a small amount of return ammonia gas.
  • Outlet NH 3 concentrations (mol%) of the ammonia synthesis column (reactor) 13 in the present invention and the conventional example were 25 mol% and 20 mol%, respectively.
  • the amount in the present invention is 1.2.
  • the raw material gas (hydrogen (H 2 ) and nitrogen (N 2 )) 11 for ammonia synthesis is introduced into the ammonia synthesis column 13.
  • the return raw material gas 11B which has been returned by the raw material return line L 12 is introduced.
  • the synthetic gas 14 containing the ammonia gas 12A synthesized in the ammonia synthesis column 13 and the unreacted raw material gas 11A is cooled to about 30 to 50°C by the water-cooled cooler 16 with the coolant 15, disposed in the discharge line L 11 .
  • the synthetic gas 14A after cooling is introduced into the ammonia separator 17, and the ammonia gas 12A and the liquid ammonia 12B are separated from each other here.
  • the separated liquid ammonia 12B is recovered as a product ammonia.
  • the raw material gas containing the ammonia gas 12A separated by the ammonia separator 17 is returned to the ammonia synthesis column 13 as the return raw material gas 11B by the raw material return line L 12 , and ammonia synthesis is performed again here.
  • the return raw material gas 11B is compressed to a predetermined synthesis pressure by the compressor 18 disposed in the raw material return line L 12 .
  • the synthetic gas 14 is cooled by the water-cooled cooler 16 or the air-cooled cooler 22. Therefore, the ammonia concentration in the return raw material gas 11B returned to the ammonia synthesis column 13 is as high as 5 mol% or more, but a ruthenium catalyst is used as an ammonia synthesis catalyst that synthesizes the ammonia gas 12A in the ammonia synthesis column 13, and therefore the reaction activity is improved.
  • the raw material gas 11 is introduced into the raw material return line L 12 prior to the compressor 18 as a make-up gas through the make-up gas line L 14 to be mixed with the return raw material gas 11B, as needed, so as to obtain a predetermined synthesis concentration in the ammonia synthesis column 13.
  • the ammonia synthesis method of the present invention includes the following ammonia synthesis loop steps.
  • a first step is an ammonia synthesis step of synthesizing the ammonia gas 12A from the raw material gas (hydrogen and nitrogen) 11 for ammonia synthesis.
  • a second step is a water-cooled or air-cooled cooling step of cooling the synthetic gas 14 containing the obtained ammonia gas 12A and the unreacted raw material gas 11 with the coolant 15 or the air 21.
  • a third step is an ammonia separation step of separating the synthetic gas 14A after water-cooling is separated into the ammonia gas 12A and the liquid ammonia 12B.
  • a fourth step is a compression step of compressing the return raw material gas 11B when the raw material gas containing the separated ammonia gas 12A is returned to the ammonia synthesis step side as the return raw material gas 11B.
  • the ammonia concentration in the return raw material gas 11B to be introduced is 5 mol% or more, and a ruthenium catalyst is used as an ammonia synthesis catalyst that synthesizes the ammonia gas 12A. Therefore, even when the temperature of the synthetic gas 14A after cooling in the water-cooled or air-cooled cooling step of the second step is from 30 to 50°C, much higher than the conventional temperature of 10°C or lower, it is possible to reduce refrigerant manufacturing cost without using a product ammonia as a chiller refrigerant and to improve an operating efficiency of ammonia synthesis.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Thermal Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Combustion & Propulsion (AREA)
  • General Chemical & Material Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Catalysts (AREA)

Claims (1)

  1. Verfahren zur Synthese von Ammoniak, umfassend:
    einen Ammoniak-Syntheseschritt in Form des Synthetisierens eines Ammoniakgases (12A) aus einem Rohmaterialgas (11) für die Ammoniaksynthese, wobei es sich bei einem das Ammoniakgas (12A) aufbauenden Ammoniaksynthesekatalysator um einen Rutheniumkatalysator handelt;
    einen Wasserkühlungs- oder Luftkühlungsschritt in Form des Wasserkühlens oder Luftkühlens eines Synthesegases (14), welches das erhaltene Ammoniakgas (12A) und ein nichtumgesetztes Rohmaterialgas (11A) enthält;
    einen Ammoniak-Auftrennungsschritt in Form des Auftrennens des Synthesegases nach dem Kühlen (14A) in das Ammoniakgas (12A) und flüssigen Ammoniak (12B); und
    einen Verdichtungsschritt in Form des Verdichtens eines Rohmaterialrückgases (11B), wenn das das abgetrennte Ammoniakgas (12A) enthaltende Rohmaterialgas als Rohmaterialrückgas (11B) an den Ort des Ammoniak-Syntheseschritts zurückgeführt wird,
    dadurch gekennzeichnet, dass die Ammoniakkonzentration in dem Rohmaterialrückgas (11B), welches in den Ammoniak-Syntheseschritt einzubringen ist, 5 Mol% oder mehr beträgt und die Temperatur des Synthesegases nach dem Kühlen (14A) von 30 bis 50°C beträgt.
EP15837863.8A 2014-09-05 2015-04-21 Verfahren für ammoniaksynthese Active EP3190088B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2014181614A JP6399867B2 (ja) 2014-09-05 2014-09-05 アンモニア合成システム及び方法
PCT/JP2015/062098 WO2016035376A1 (ja) 2014-09-05 2015-04-21 アンモニア合成システム及び方法

Publications (3)

Publication Number Publication Date
EP3190088A1 EP3190088A1 (de) 2017-07-12
EP3190088A4 EP3190088A4 (de) 2017-08-09
EP3190088B1 true EP3190088B1 (de) 2019-05-29

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US (1) US10246340B2 (de)
EP (1) EP3190088B1 (de)
JP (1) JP6399867B2 (de)
DK (1) DK3190088T3 (de)
WO (1) WO2016035376A1 (de)

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WO2020085324A1 (ja) 2018-10-23 2020-04-30 つばめＢｈｂ株式会社 アンモニア合成システムおよびアンモニアの製造方法
CN109646984A (zh) * 2019-01-17 2019-04-19 南京工业大学 一种具备储冷功能的VOCs多级冷却回收系统
CN112299446A (zh) * 2019-07-24 2021-02-02 曹为平 开放式合成氨系统

Family Cites Families (10)

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Publication number Priority date Publication date Assignee Title
CA1229485A (en) 1984-01-23 1987-11-24 Toyo Engineering Corporation Process for refining an ammonia synthesis gas
JPS61106403A (ja) 1984-10-30 1986-05-24 Toyo Eng Corp アンモニア合成ガスの精製法
US4568530A (en) * 1984-10-16 1986-02-04 The M. W. Kellogg Company Ammonia synthesis
JPH11304283A (ja) 1998-04-20 1999-11-05 Chiyoda Corp アンモニア合成装置における冷凍システム
US6171570B1 (en) * 1998-10-12 2001-01-09 Kellogg Brown & Root, Inc. Isothermal ammonia converter
JP2003020221A (ja) * 2001-07-05 2003-01-24 Nkk Corp アンモニア水製造装置
EP1375418A1 (de) * 2002-06-28 2004-01-02 Ammonia Casale S.A. Verfahren und Vorrichtung zur Herstellung von Ammoniak-Synthesegas
DE60304257T2 (de) 2002-07-11 2006-08-31 Haldor Topsoe A/S Verfahren zur Herstellung von Ammoniak sowie Katalysator hierzu
US7371361B2 (en) * 2004-11-03 2008-05-13 Kellogg Brown & Root Llc Maximum reaction rate converter system for exothermic reactions
JP2014162662A (ja) * 2013-02-21 2014-09-08 Mitsubishi Heavy Ind Ltd アンモニア合成システム及び方法

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Publication number Publication date
WO2016035376A1 (ja) 2016-03-10
EP3190088A1 (de) 2017-07-12
US10246340B2 (en) 2019-04-02
JP6399867B2 (ja) 2018-10-03
EP3190088A4 (de) 2017-08-09
JP2016056039A (ja) 2016-04-21
DK3190088T3 (da) 2019-09-02
US20170283271A1 (en) 2017-10-05

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